Process for adding lead to cotton by use of reaction between deae cellulose and alkaline solution of sodium plumbite

ABSTRACT

THIS INVENTION RELATES TO A PROCESS FOR ADDING LEAD TO CELLULOSIC FABRIC BY REACTING DIETHYLAMINOETHYTL (DEAE) CELLULOSE WITH AN ALKALINE SOLUTION OF SODIUM PLUMBITE.

United States Patent 3,563,688 PROCESS FOR ADDING LEAD TO COTTON BY USE OF REACTION BETWEEN DEAE CELLULOSE 13H 1;: ALKALINE SOLUTION OF SODIUM PLUM- Truman L. Ward and Ruth R. Benerito, New Orleans,

La., assignors to the United States of America as represented by the Secretary of Agriculture No Drawing. Filed May 27, 1969, Ser. No. 828,331

Int. Cl. D06m 1/00 US. Cl. 8116 2 Claims ABSTRACT OF THE DISCLOSURE This invention relates to a process for adding lead to cellulosic fabric by reacting diethylaminoethyl (DEAE) cellulose with an alkaline solution of sodium plumbite.

A non-exclusive, irrevocable, royalty-free license in the invention herein described, throughout the World for all purposes of the United States Government, with the power to grant sublicenses for such purposes, is hereby granted to the Government of the United States of America.

Prior art processes are known for the preparation of diethylaminoethylated cellulose. Prior art processes are also known for the preparation of strong base anion exchangers to partially convert diethylaminoethylated cellulose to the quaternary form by refluxing in 10% CH I in absolute alcohol.

In contrast to the prior art, this invention relates to a process whereby lead is added to diethylaminoethyl cellulose to produce a fabric white in color with improved weathering characteristics in air and soil and may serve as a mild radiation barrier.

By the preferred process of this invention, DEAE cellulosic fabric is reacted at room temperature for 3 to 24 hours with an 8 to 20% aqueous sodium hydroxide solution saturated with sodium plumbite. After reaction, the fabric is washed with water, dried, and equilibrated.

The tertiary amine group is apparently necessary to the reaction because lead does not add, under the same conditions, to either plain cellulose or cellulose containing primary or secondary amine groups, or to quaternized DEAE cellulose.

The following examples illustrate but do not limit the scope of this invention. All percentages are by weight.

EXAMPLE 1 A 12 inch square of 80 x 80 DEAE cotton fabric (0.8% N) weighing approximately 10 g. was immersed for 4 hours in a 15 weight percent aqueous sodium hydroxide solution which had been saturated with sodium plumbite. After reaction the fabric was washed thoroughly with water, dried, equilibrated, and analyzed. The fabric contained 7.26% lead. After boiling for one hour in a solution of Alconox detergent in water, the fabric was washed, dried, equilibrated and analyzed. The fabric analyzed 6.91% lead.

EXAMPLE 2 Example 1 except DEAE fabric containing 1.0% N was substituted for the starting fabric. 6.48% Pb was added.

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EXAMPLE 3 Example 1 except DEAE fabric containing 0.44% N was substituted for the starting fabric. 7.64% P'b was added.

EXAMPLE 4 Example 1 except DEAE fabric containing 0.81% N was substituted for the starting fabric. 7.60% Pb was added.

EXAMPLE 5 Example 2 except a 20% NaOH solution was used rather than 15 7.24% Pb Was added.

EXAMPLE 7 Example 1 except a series of NaOH solutions of different concentrations used instead of 15% and three hours reaction time was used.

Percent Reaction P time,

Percent NaOH added hours EXAMPLE 8 Example 8 except 24 hours reaction time used.

Percent NaOH: Percent Pb added We claim:

1. A process for adding lead to a diethylaminoethylated cellulose fabric which process comprises:

(a) reacting a diethylaminoethylated cellulose fabric at room temperature for a period of about 3 to 24 hours with an 8 to 20 weight percent aqueous sodium hydroxide solution saturated with sodium plumbite, and

(b) washing the fabric free of excess reagents.

2. The product produced by the process of claim 1.

References Cited Guthrie, Industrial and Engineering Chemistry, pp. 21872189, September 1952.

Benerito, Textile Research Journal, vol. 38 pp. 279- 292 (1968).

GEORGE F. LESMES, Primary Examiner I. CANNON, Assistant Examiner US. Cl. X.R. 260-2.1, 232 

